Abstract
Total reflection X-ray fluorescence spectrometry (TXRF) offers the possibility of simple and precise multielement determination of trace element impurities in ultrapure regents. With little expenditure of time and sample preparation—30 min for sample preparation and measurement are usual—as well as the small sample volumes involved, 100 μl of sample material are sufficient for a complete multielement determination, detection limits in the range of 20–100 pg ml have been obtained. Adapting a simple evaporation step for pre-concentration, the limits of detection can be improved to below 5 pg ml . The precision is in the range of 5–20%. The reliability of the sample preparation procedures and the accuracy of the results are checked by recovery investigations and by independent analysis of duplicate samples using ICP-MS. Results obtained for commercial products, such as HF, HCl, HNO 3, H 2SO 4, NH 4F and NH 3, are presented and are compared to those obtained after additional purification.
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